3m advanced materials division 3m™ nextel™ 610 towpreg: a ...€¦ · • matt warnock • andy...

1© 3M 2020. All Rights Reserved.

US Advanced Ceramics Association

44th Annual Conference on Composites, Materials, and Structures

Cocoa Beach, FL

Jan 27, 2020

3M™ Nextel™ 610 Towpreg: A new pathway for oxide ceramic matrix composite fabrication

3M Advanced Materials Division

Aaron Beaber, Amor Calubayan, Daimon Heller, Kari McGee, Amit Patel, James Reimer, and Henrik van Lengerich3M CompanySt. Paul, MN

Eric Bonebrake and Scott DigiorgioElectroImpactMukilteo, WA

DisclaimersExport Control – Nextel is controlled for export by the U.S. Department of Commerce and cannot be transferred to any non-U.S person or non-U.S. location without further license or license exception.

Experimental material – Any technical information, recommendations, and other statements contained in this document or provided by 3M personnel about experimental material are based on limited information and the accuracy or completeness of such information is not guaranteed.


Automated fiber placement

• Automated Fiber Placement (AFP) is a digital additive

manufacturing process where multiple tows can be

independently added or cut in the fabrication of a composite

• AFP combines the advantages of

Filament winding + automated tape layup + 3D printing

Technique Fabrication rates Geometric constraints

Filament winding FastRequires constant convex

curvature

Automated tape layup FastSimple shapes with no compound curvature

3D printing Slow Minimal

Automated fiber placement FastLower contour parts and

male tools


Fabrication of composites using AFP

Advantages vs hand layup

• Lower scrap

• Lower material costs

• Automated process• More consistent and higher quality parts

• High layup rates

• Digital process (inspection, digital twin, etc)

• Process scales and is flexible• Many different part geometries and sizes can be

produced via the process

Limitations

• Better suited for lower contour parts and male tools

• Minimum feature size• Radius ≥500 mm for 180° tool

• Minimum part size• Min segment length of 4”

Potential applications for CMC structures

• Thermal shielding

• Exhaust cone

• Combustion liner

4© 3M 2020. All Rights Reserved. 4

3M™ Nextel™ 610 Towpreg – Experimental Product

Nextel 610 Spread tow• Controlled width and thickness• Water soluble sizing

Release liner• Polyethylene• Carrier for tacky towpreg

Ceramic matrix• All alumina, water based composition• Organic additives to provide tack

Coating• Slurry infused into fiber tow to provide

controlled matrix content• Water soluble sizing removed

from fiber surfaces

Drying• Water removed from slurry to produce

a dry matrix• Target < 1 wt.% water

• Room temperature stable matrix• Humidity can result in slightly

higher moisture content(1.5 to 2 wt.%)

Winding• Level wound roll• Interleaved liner

• Smooth, stable unwind of dry towpreg


3M™ Nextel™ 610 Towpreg – Experimental Product

Nextel 610 Towpreg• Controlled width and thickness• Controlled matrix content

• Dry, room temperature stable• Heat-activated tack

Fiber Nextel 610Denier (g/9,000m) 10,000

Nominal width (mm) 6.35Nominal thickness (um) 200

Ceramic matrix content (wt%) 51Oxide particle composition alumina

Liner polyethylene

Towpreg properties are representative and not for specification purposes

Towpreg cross section


A new pathway for simple geometry parts

• We are enabling another, more simple supply chain with a potential for the lowest cost RM for oxide CMCs

• Enables customers to pursue lower cost manufacturing, including AFP, for simple geometries

Fiber manufacturing

Sizing application

WeavingSizing removal

(Burn off)

Fabric prepreg model

Prepregging Part layup Firing

Fiber manufacturing

Fiber spreading

Towpreg manufacturing

Part layup Firing

Tow preg enabled model

7. All Rights Reserved.15 April 2020© 3M

Panel fabricationPoor tack Excellent tack

✓

Nextel layup rates on flat part Ply #1: 100-200 in/min

≥Ply #2: 800-1000 in/minOptimized carbon typically runs at 3000 in/min

(qualified production rate)

Early prototypes showed insufficient tack and peeled up after placement

IR heater applying heat to the part during material layup


Physical and mechanical properties

Fiber orientation 0/90 cross-plyPly count 20

Per ply thickness (mm) 0.11Fiber content (vol%) 41.3Areal density (gsm) 303

Tensile strength (MPa) 290Tensile modulus (GPa) 108

Flex strength (MPa) 382Flex modulus (GPa) 122

Interlaminar shear strength (MPa) 20

Towpreg composite properties are representative and not for specification purposes

Sintered panel polished cross sectionTest panels were fabricated with Nextel Towpreg using AFP.Measured properties are given below. The image to the rightshows the cross section of the composite, highlighting theconsistent distribution of fiber and matrix throughout thecomposite.


Room temp performance comparison

Material 3M CHI Axiom COIC WPX Keramikblech

Fiber N610 N610 N610 N610 N610 N610

Matrix aluminaalumina-

silicaalumina-

silicaalumina-

silicaalumina

alumina-zirconia

Fiber content (vol%)

41 41 46 40 39 42

Porosity (vol%)

27 23 21 26 28

SourceUSACA 2020

USACA 2017

NSMMS 2019

HTCMC 2019

whipox.com HTCMC 2019

0

20

40

60

80

100

120

Ten

sile

mo

du

lus

(GPa

) Tensile modulus (GPa)

0

5

10

15

20

25

Inte

rlam

inar

sh

ear

stre

ngt

h(M

Pa)

Interlaminar shear strength (MPa)

050

100150200250300350

Ten

sile

str

engt

h (

MPa

) Tensile strength (MPa)

Compared to other commercial CMCs, composites generated with Nextel Towpreg using AFP show in family performance at room temperature.

10All Rights Reserved.15 April 2020© 3M

Steering trials

• Steering evaluated with arcs of Nextel Towpreg on carbon and PET substrates• Evaluation of radius from 500-2500 mm• No defects for radius greater or equal to 1000 mm

• As a comparison, optimized carbon typically runs at 2000 mm for ¼”

Buckles/bubbles

wrinkles

Examples of steering defects


Complex geometries

• 20” diameter, 22” height demo cone• Multiple layup configurations

evaluated (0°, 90°, 45°, 30°, etc)

0° 45°

Cone Angled radius

20 mm120°

30 mm120°

40 mm120°

10 mm90°

20 mm90°

• 5 sided tool to represent multiple features relevant to CMC fabrication

• 90° and 120° features ranging from 10-40 mm radius • Layup orientation: 0° / +45° / -45°

A variety of tooling has been explored to identify capabilities and limitations of the Nextel Towpreg with AFP


Angled tool trials

• 90° and 120° features ranging from 10-40 mm radius • Tool wrapped with polyimide film (gold color)• Layup orientation: 0° / +45° / -45°• 22 plys

Example of 120°, 30 mm radius layup


Angled tool layup results – 90° radius

20 mm

10 mm

Ply 4: 0° Ply 5: +45° Ply 6: -45°radius

Minor defects observed during layup, mostnotably in 45° plys. These could likely becorrected with additional AFP tuning.


Composite processing – CT analysis – 10 mm, 90°

Layup Autoclaved Sintered

Thickness measurements

Representative thickness slice and measurement positions (#1-7)

Parts were scanned using CT after layup, autoclaving, and sintering process steps. Thickness was measured at 7 positions along the part profile and reported as an average along the length of the part.

1

2

34

5

6

7

Grid of measurement locations


Wrinkling defect

• Wrinkle observed in both 10 and 20 mm parts (red arrow)

• Likely the result of excessive part contraction during consolidation

• Using thickness measurements, a bulk factor of 130-140% was calculated. Plot to the right shows bulk factor for each measurement location across the part profile.

• High bulk factor can be addressed through

• AFP parameters

• Tooling / debulking

• Towpreg formulation

10 mm / 90° 20 mm / 90°

100%

110%

120%

130%

140%

150%

160%

0 1 2 3 4 5 6 7 8

bu

lk f

acto

r (%

)

position (arb)

10mm

20mm


Challenges with AFP rollers – Metal abrasion Driven feed roll (440C SS) Passive feed roll (Bronze 954)

Black contamination on panels (red arrows) identified as:• Copper from passive rollers• Iron from active rollers

Potential solution: PVD coated rollers

Coating polished, but much less debris observed on panels

Drive rolls polished by processing Nextel Towpreg

Conclusions

• Introducing a new experimental product: Nextel 610 Towpreg

• Unique dry matrix providing room temperature stability and heat-activated tack

• AFP compatibility

• In family room temperature mechanical performance

Next steps

• Continue to evaluate product performance, including small volume sampling

• Process window/constraints for AFP

• Demonstration part(s), in-service testing

• Composition/construction development

• Mechanical data set for elevated temperature performance

All Rights Reserved.15 April 2020© 3M

s

To learn more, contact:

Aaron Beaber, Product Developer ([email protected])Clara Choe, Business Development Manager ([email protected])Ceramics Platform3M Advanced Materials Division

3M

• Myles Brostrom

• Darin Erickson

• Mary Kostuch

• Alejandro Munoz

• Lars Poppy

Acknowledgements

ElectroImpact

• Kyle Jeffries

• Matt Warnock

• Andy Purvis

s

DisclaimersImportant Notice and Disclaimer: This 3M product is an experimental or developmental product that has not been introduced or commercialized for general sale, and its formulation, performance characteristics and other properties, specifications (if any), availability, and pricing are not guaranteed and are subject to change or withdrawal without notice. User is solely responsible for evaluating the 3M product and determining whether it is fit for a particular purpose and suitable for users method of application. User is solely responsible for evaluating third party intellectual property rights and for ensuring that users use of 3M product does not violate any third party intellectual property rights. This 3M product is sold or made available “AS IS.” 3M MAKES NO WARRANTIES OR CONDITIONS, EXPRESS OR IMPLIED, INCLUDING, BUT NOT LIMITED TO, ANY IMPLIED WARRANTY OR CONDITION OF MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE OR ANY IMPLIED WARRANTY OF NON-INFRINGEMENT OR ANY IMPLIED WARRANTY OR CONDITION ARISING OUT OF A COURSE OF DEALING, CUSTOM OR USAGE OF TRADE.

Limitation of Liability: Except where prohibited by law, 3M will not be liable for any loss or damages arising from the 3M product, whether direct, indirect, special, incidental or consequential, regardless of the legal theory asserted, including warranty, contract, negligence or strict liability.

Technical Information: Technical information, recommendations, and other statements contained in this document or provided by 3M personnel are basedon limited information and the accuracy or completeness of such information is not guaranteed. Such information is intended for persons with knowledge and technical skills sufficient to assess and apply their own informed judgment to the information. No license under any 3M or third party intellectual property rights is granted or implied with this information.

Export Control: The 3M product(s) listed here may be controlled commodities under applicable U.S. export control laws and regulations, including, but not limited to, the U.S. International Traffic in Arms Regulations (ITAR) and the Export Administration Regulations (EAR). These laws and regulations may, among other things, prohibit the export and/or reexport of controlled product(s) to any or all locations outside of the United States without prior U.S. Government export authorization, the sharing of export controlled technical data and services with those anywhere who are not U.S. citizens or U.S. permanent residents, dealings with U.S. Government, United Nations and other "Restricted Parties," and proliferation activities including those that further nuclear, chemical, or biological warfare, missile stockpiling/use, or the use of rockets or unmanned aerial vehicle systems. 3M and purchasers or prospective purchasers of the 3M product(s) shall comply with all applicable export control laws and regulations, which may require obtaining and maintaining applicable export control authorization or licenses, and understand that the ability of a party to obtain or maintain such authorization or license is not guaranteed. The exporter of record has the sole responsibility to determine whether the export or subsequent reexport of the 3M product(s) requires export authorization. An explicit condition to 3M selling or making available the 3M product(s) is the customer's agreement to comply with all applicable trade compliance laws and regulations.

3m advanced materials division 3m™ nextel™ 610 towpreg: a ...€¦ · • matt warnock • andy...

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